Hitachi HF2000 TEM Manual de usuario

HITACHI HF2000 TEM

Operation Manual

- Alignment and Operation -

Dear users,

To help you have a smooth and successful TEM observation, I wrote up this basic operation manual.

Systematic theoretical training plus hands-on practical training may be the best way to understand the

details of this operation instruction for HF2000 TEM.

There are some notes in this instruction. Please read and follow them carefully, and please make sure you

follow what I told you ask before you touch the TEM if you do not know the consequence of your action.

Takamichi MIYAZAKI / June 2009

Contents

1. Startup

2. Set the sample (loading)

3. Applying High Voltage

4. Prepare for beam alignment

5. Correct condenser astigmatism

6. Z-height adjustment

7. Voltage center

8. Image focus and Objective lens astigmatism correction

9. Selected area electron diffraction

10. Bright field imaging

11. Photographing

12. CCD camera

13. Sample tilt

14. Astigmatism correction of beam tilt

15. High resolution imaging

16. Microbeam diffraction

17. Sample exchange (unloading)

18. Shutdown

19. Film exchange

1. TEM startup

•Check the comments in the TEM log book. Enter your name,

laboratory and contact information on the log book before any

action on the TEM.

•Make sure that TEM vacuum is good. At the vacuum state

(right panel), SPEC, COL, and CAM indicators should be

VAC position (all green), and GUN indicator is at EVAC

position (green flashing).

•Make sure that TEM is set at standby positions:

a) OBJ. TEMP. MONITOR: 210C and below

b) Objective, selected area and condenser apertures are out (position 0).

c) GV (Gun Valve) is Closed

d) ACC. VOLTAGE: off; HV: on at 200kV

e) Sample position: X = 0, Y = 0; Sample tilts: 0

f) Bright/Dark field selector set at Bright field.

g) Microscope is at [ANA1] mode.

h) Magnification: 1000K – 1500K

i) Normally, the sample holder stays TEM. It is situated at position A

j) Lens Current (C1, C2, OBJ) : not 0

k) Unexposed film number: 50 FULL

Film number: 1 0

•After confirmation of the standby positions, enter chiller temperature and pressure, COMPR pressure,

HV tank pressure, and vacuum state on the log book.

Position A

EVAC

Selected Area

diffraction aperture

Objective aperture

Correct condenser

erture

X-ray detector

erture

Right main panel

Vacuum state

2. Set the sample (loading)

Normally, the sample holder stays in TEM. It is situated at position A (see in the following diagram).

Note: Objective aperture must be out during sample holder loading / unloading.

•Turn the switch on goniometer to Air. Wait till SPEC is at Air position (red light on vacuum state) and

pull the holder out.

•The sample is securely seated in the holder

•Loading sample holder into TEM

Follow the route indicated in the diagram below to load

your sample holder into the TEM.

1) Insert the sample holder horizontally along and

press it, then turn the switch to EVAC.

2) When electron sound rings, turn the holder clockwise till it stops.

3) Let the sample holder go into the TEM horizontally along and smoothly. The sample

holder must be under control.

4) Turn the sample holder counter-clockwise till it stops

5) Let the holder go into the TEM fully.

B位置

C位置

A位置

（EVAC⇔

IR）

Ｂ

位置

A位置

Ｂ位

置

Bposition

Aposition

Cposition

Aposition

Bposition

EVAC / AIR

3. Applying HV

•Apply HV when vacuum is good

•Make sure that the applying HV conditions are set at following state:

V0 VOLTAGE 200kV

RRATIO 5.5

I1 CURRENT 30µA

•Press the [FE] bottom once (left panel) and press [FLASH] when it’s flashing. IF current rise up, if the

IF current is lower than 0.30 mA, repeatedly press [FLASH] bottom till IF current is > 0.30mA.

•After IF current exceeds 0.30mA, wait till V0 VOLTAGE rises up to 200kV. Then V1 and V2 Voltage

rises gradually up to the setting value (watch the ACC VOLT on the CRT monitor).

•Enter the V1 Voltage and IF current on the log book (Yellow book).

********************************************************************************

When the emission current drops below 10µA, press [I1C] and recalibrate extraction voltage to raise the

emission current to 30µA. The beam wander off during the process but return by the end of the I1C state.

Repeat alignment procedure because the changed extraction voltage affects the caustic.

********************************************************************************

4. Prepare for beam alignment

•Press [ANA1] to change selected mode: Analysis →TEM mode.

•Reset switch (Red square button)

[I1C]

[FLASH]

Left main panel

5. Correct condenser astigmatism（Magnification : 100K ~ 200K）

Be sure to use the correct condenser astigmatism for TEM mode:

•Open the GV and make sure you hear it click open.

•Turn the Brightness control (left panel) to crossover, and center the beam with the Brightness

Centering knobs (right panel).

•Using the condenser stigmator (right sub panel) make the caustic as round or axial symmetry. And

using the 3rd order stigmator (left sub panel) makes the caustic as symmetry. The 3rd order correction

will be slight and the controls should be close to the center positions.

•The correctly aligned caustic will appear as a circle with Star in TEM mode. The image is shown

below.

•Insert condenser aperture (First aperture) and

minimize the swinging beam using the condenser

X/Y adjustment screws when passing through

crossover.

3rd Cond Stig

2nd Cond Stig

3rd Cond stigmator

2nd Cond stigmator

6. Z-height adjustment

•Move edge of sample and set the objective lens current to 5.72 using focus control. Focus the sample

using the Z-height adjustment screw on the specimen holder entry port.

Note: An objective lens current of 5.72 is the optimal setting for minimum spherical aberration.

You may also focus sample using wobblers method or minimum contrast method for the image

focus.

7. Voltage center

•Move edge of sample.

•Turn on [HVM] (HV MODULATION, right panel). The image feature may oscillate.

•Adjust BEAM TILT (right sub panel) to minimize the vibration of the feature.

•Turn off [HVM] (right panel).

•Repeat the alignment procedure a few times because the beam tilt and objective stigmatism correction

have disturbed the condenser stigmatism corrections. In general, completing the alignment procedure

twice will be sufficient.

Z-height adjustment

左サブパネル

8. Astigmatism correction of objective lens

•Reset the OBJ STIGM-X and Y control knobs (stigmator)

on the left sub panel.

＊This returns setting to the stigmator to preset level.

•Set a magnification 2 or 3 times higher than used for

photographing.

•Turn the focus control knob clockwise so as to obtain

slightly over-focused image, and a fringe appears outside

the collodion hole.

•Adjust the OBJ STIGM-X and Y control knobs so that the width of the fringe outside the collodion

hole becomes uniform.

•Manipulate the focus control knob so as to approach just focus from over-focus in order to narrow the

fringe width.

•Find a as granularity a amorphous as possible and adjust the OBJ STIGM-X and Y control knobs so

that granularity a amorphous becomes finer granularity as shown in the figure below.

9. Image focus and Objective lens astigmatism correction

(Including Selected area electron diffraction (SAED))

This is to tell you how to correct objective lens astigmatism using amorphous film which is useful in

recording a high resolution image.

•Center a small hole / particle / the sharp edge of sample.

•Insert and center a suitable Selected Area (SA) aperture.

•Press [DIFF] (left panel) and set the camera length to 0.80m using Magnification knob. If the central

spot (transmitted wave) is still disk, focus the pattern by adjusting Diffraction Spot (left panel).

Note: Open the beam to form a parallel illumination on the sample by turning Brightness

clockwise. Diffraction spots will become weaker and smaller. If the central spot is disk instead of

a spot, adjusting Diffraction Spot is needed.

Left sub panel

•Insert objective aperture into the central spot that should be centered by using the objective X/Y

adjustment screws.

•Press [ZOOM] to seen a bright field image.

•Pull out SA aperture

•Correct the astigmatism by adjusting fine focus and OBJ STIG X and Y controls if necessary.

(Using minimum contrast method and amorphous contrast)

10. Bright fielding imaging

•Find an interesting sample area.

•Focus the beam and sample to the crossover.

•Press [DIFF]. (see Sec.9, SAED)

Note: If the central spot is not at the viewing center, center it using the INTER ALIGN X and Y knobs

(left sub panel). If the spot is not round, make it round using INTER STIG X and Y knobs (left sub

panel).

•Insert the objective aperture into the beam by turning the aperture handle clockwise.

•Press [ZOOM] to see a bright field image.

•Adjust fine focus and OBJ STIG if necessary.

•Adjust Brightness so that Auto exposure time is between 2-5 seconds.

•Cover the viewing window

•Press [Photo] to expose the film and record a bright field image.

電子回折図形

明視野像

格子（多波干渉）像

Bright fielding imaging

Electron diffraction pattern

Lattice imaging

11. Photographing for film

Usage of auto exposure time set mode

Time mode provides a function for automatically setting the exposure time so as to obtain optimum

photographic density on a film in response to a determined brightness.

•Set the exposure time setting knob at AUTO.

•Press the PHOTO key to start film exposure.

Manual mode

•Set a desired exposure time by turning the EXPOSURE TIME control knob. The set exposure time is

displayed at the bottom right on the CRT.

•Optimum exposure time lines for

Bright field image: 1 to 4 seconds

Dark field image: 12 to 30 seconds

Selected area diffraction pattern: 0.5 to 1 seconds

Nano beam diffraction pattern: 8 to 16 seconds

•Press the PHOTO key to start recording

12. CCD camera

•Turn on the power to TV monitor and control.

•Open the beam by turning Brightness clockwise. Brightness will become weaker.

Note: Do not use CCD camera for diffraction pattern, low-magnification image and direct beam.

•Cover the viewing window.

•Press [STOP] and [PHOTO].

13. Sample tilt

•Press [DIFF]. (see Sec.9, SAED)

•Adjust the sample tilt with electron beam direction along the zone axis.

14. Astigmatism correction of beam tilt

•Turn the WOBBLER ANGELE control on the right main panel fully clockwise.

•Press the WOBBLER ON/OFF switch.

•When astigmatism is not corrected, rotating motion in a specific direction is observed. Adjust the

[BTX] and [BTVX] controls on the left sub panel so that non-directional image rotation is observed as

shown below.

•Turn the WOBBLER ANGELE control counterclockwise by 3 steps. When astigmatism is not

corrected, adjust the [BTY] and [BTVY] controls on the left sub panel so that non-directional image

rotation is observed as shown below.

FOOT

RIGHT

FOOT

LEFT

HAND

LEFT

HAND

RIGHT

FOOT

RIGHT

HAND

LEFT

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